ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Acetic Acid → 3'-(4-Fluorophenyl)-4-[2-(1,3,5-trimethyl-1H-pyrazol-4-yl)-ethyl]-3,4,5,6-tetrahydro-2H-[1,2']bipyrazine hydrochloride

HRID 220501
ノート
印刷プレビュー

反応式

HRID 220501 の反応式
[CH3:1][N:2]1[C:6]([CH3:7])=[C:5]([CH2:8][CH:9]=O)[C:4]([CH3:11])=[N:3]1.[F:12][C:13]1[CH:18]=[CH:17][C:16]([C:19]2[C:20]([N:25]3[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]3)=[N:21][CH:22]=[CH:23][N:24]=2)=[CH:15][CH:14]=1.C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(Cl)[Cl:50]>>[ClH:50].[F:12][C:13]1[CH:18]=[CH:17][C:16]([C:19]2[C:20]([N:25]3[CH2:26][CH2:27][N:28]([CH2:9][CH2:8][C:5]4[C:4]([CH3:11])=[N:3][N:2]([CH3:1])[C:6]=4[CH3:7])[CH2:29][CH2:30]3)=[N:21][CH:22]=[CH:23][N:24]=2)=[CH:15][CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 5

HCID 176Acetic AcidHCID 6344DichloromethaneHCID 5049666Sodium triacetoxyborohydrideHCID 64868769(1,3,5-Trimethyl-1H-pyrazol-4-yl)-acetaldehydeHCID 673669592-(4-Fluorophenyl)-3-(piperazin-1-yl)pyrazine

生成物 1

HCID 68594264
3'-(4-Fluorophenyl)-4-[2-(1,3,5-trimethyl-1H-pyrazol-4-yl)-ethyl]-3,4,5,6-tetrahydro-2H-[1,2']bipyrazine hydrochloride
収率 5%

実験手順

Combine (1,3,5-trimethyl-1H-pyrazol-4-yl)-acetaldehyde (0.35 g, 2.27 mmol) and 3′-(4-fluorophenyl)-3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl (0.71 g, 2.76 mmol) in DCM (10 mL) and stir at room temperature for 10 min. Add glacial acetic acid (0.21 mL, 3.44 mmol) followed by sodium triacetoxyborohydride (0.73 g, 3.44 mmol). Stir at room temperature for 2 hr. Concentrate, dissolve in methanol (5 mL) and load on a 10 g SCX column. Wash with methanol (2×50 mL). Elute with 2 M ammonia in methanol (2×30 mL). Concentrate the eluent and purify (silica gel chromatography, eluting with 45:45:10 hexanes:DCM:ethanol), to give the free base of the title compound (48 mg, 5%). Dissolve the free base (0.041 g, 0.104 mmol) in methanol and add a solution of ammonium chloride (0.006 g, 0.104 mmol) in a minimal volume of methanol. Shake for 18 hr. at room temperature and concentrate to give the title compound (50 mg, 95%). MS (ES): m/z=395 [M+H]+.

後処理

  1. concentrationConcentrate
  2. dissolutiondissolve in methanol (5 mL)
  3. washWash with methanol (2×50 mL)
  4. washElute with 2 M ammonia in methanol (2×30 mL)
  5. concentrationConcentrate the eluent
  6. custompurify
  7. wash(silica gel chromatography, eluting with 45:45:10 hexanes:DCM:ethanol)

出典と根拠

ORDレコード
ord-da2f02fbfd7d4e56997e4f3c6b9bb55d
出典データセット
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08202873B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート